CN113732301B - 3DP preparation technology for improving strength and corrosion resistance of magnesium alloy - Google Patents
3DP preparation technology for improving strength and corrosion resistance of magnesium alloy Download PDFInfo
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- CN113732301B CN113732301B CN202111082012.XA CN202111082012A CN113732301B CN 113732301 B CN113732301 B CN 113732301B CN 202111082012 A CN202111082012 A CN 202111082012A CN 113732301 B CN113732301 B CN 113732301B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/10—Formation of a green body
- B22F10/14—Formation of a green body by jetting of binder onto a bed of metal powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/60—Treatment of workpieces or articles after build-up
- B22F10/64—Treatment of workpieces or articles after build-up by thermal means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/20—Post-treatment, e.g. curing, coating or polishing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0005—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with at least one oxide and at least one of carbides, nitrides, borides or silicides as the main non-metallic constituents
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0036—Matrix based on Al, Mg, Be or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
- C22C32/0063—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on SiC
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention discloses a 3DP preparation process for improving strength and corrosion resistance of magnesium alloy, which comprises the following steps: 1) Uniformly mixing magnesium alloy powder, ceramic powder and carbide powder according to a proportion; 2) Introducing the shape of a product to be printed into a computer control system, and printing the mixed powder and glue obtained in the step 1) in a 3D printer in an alternate spray forming mode to obtain a blank with the required shape; 3) Drying the blank obtained in the step 2), and degreasing and sintering at 300-450 ℃ in a protective atmosphere or in vacuum; 4) Sintering the blank obtained in the step 3) at a high temperature of 580-660 ℃ in a protective atmosphere or in vacuum, and cooling to room temperature.
Description
Technical Field
The invention relates to the technical field of magnesium alloy additive manufacturing, in particular to a 3DP preparation process for improving the strength and corrosion resistance of magnesium alloy.
Background
With the rapid development of equipment manufacturing industry, the demand for light weight is increasing, and magnesium alloy is used as the lightest commercial structural material, and the required field is increasing. However, with further light weight requirements, a large number of integral structural components are required, which are complex in shape and large in size and are difficult to manufacture using conventional manufacturing processes. Meanwhile, the magnesium alloy has the defects of poor deformability, low strength and poor corrosiveness, so that the application of the magnesium alloy is greatly limited.
The existing additive manufacturing technology is not limited by the shape of the formed part, so that a new technical solution is provided for the forming and manufacturing of magnesium alloy complex parts, and the application range and development space of the magnesium alloy are greatly widened. At present, the preparation technology of magnesium alloy parts with complex shapes is generally manufactured by adopting a die casting process, the subsequent further processing is required by the preparation process, the procedure is complicated, the magnesium alloy casting is obtained by adopting the die casting process, the structure of the magnesium alloy casting is polished by other equipment, and the equipment for polishing the structure of the magnesium alloy casting is complex in structure and high in price. At the same time, for parts of particularly complex shape, it is easy to cause incomplete stamping and eventually failure to obtain the desired part. This results in difficult processing, high manufacturing cost, and low production efficiency of magnesium alloy products with complex shapes, and greatly limits the application range of magnesium alloys.
Currently, magnesium alloy products manufactured using additive materials are typically lower in strength than as-cast magnesium alloys because they cannot reach a fully dense state. In addition, another fatal problem of magnesium alloy materials is that the magnesium alloy materials are not corrosion-resistant, and the current common practice is to coat a film on the surface of the magnesium alloy or add a corrosion-resistant second phase to improve the corrosion resistance of the magnesium alloy. However, after the surface is coated, the film layer is worn due to long-term use, so that corrosion still occurs. And the second phase is added in the casting process, imagination such as segregation and the like often occurs, so that the components of the final product are uneven, the performance is finally reduced, and the use requirement cannot be met.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a 3DP preparation process for improving the strength and corrosion resistance of magnesium alloy, so as to solve the problems of high difficulty, high cost and low production efficiency in manufacturing magnesium alloy products with complex structures in the prior art, and improve the mechanical strength and corrosion resistance of magnesium alloy.
In order to solve the technical problems, the invention adopts the following technical scheme:
a3 DP preparation process for improving strength and corrosion resistance of magnesium alloy comprises the following steps:
1) Uniformly mixing magnesium alloy powder, ceramic powder and carbide powder according to a proportion;
2) Introducing the shape of a product to be printed into a computer control system, and printing the mixed powder and glue obtained in the step 1) in a 3D printer in an alternate spray forming mode to obtain a blank with the required shape;
3) Drying the blank obtained in the step 2), and degreasing and sintering at 300-450 ℃ in a protective atmosphere or in vacuum;
4) Sintering the blank obtained in the step 3) at a high temperature of 580-660 ℃ in a protective atmosphere or in vacuum, and cooling to room temperature.
The invention also provides a high-strength corrosion-resistant magnesium alloy material, which is prepared by adopting the 3DP preparation process for improving the strength and corrosion resistance of the magnesium alloy, and comprises the following components in percentage by mass: ceramic powder or carbide powder 0.1-20wt% and the balance being magnesium alloy powder.
Compared with the prior art, the invention has the following beneficial effects:
the additive manufacturing process of sintering after glue bonding, printing and forming can effectively solve the problems of difficult processing of complex shapes, keep the advantage of weight reduction, have the advantages of low manufacturing cost, high production efficiency, wide application range and the like, can realize the feasibility of manufacturing large-size and complex-shape magnesium alloy workpieces, can mix other second materials in the magnesium alloy powder in any proportion, does not have the casting problems of segregation and the like, and has uniform final product components. Meanwhile, the process can densify different materials together after mixing, so that the magnesium alloy product with a complex shape can still keep higher strength and better corrosion resistance.
Drawings
The SEM pictures of the samples with different silicon carbide contents in fig. 1, wherein (1 a) is example 1, (1 b) is example 2, (1 c) is example 3, and (1 d) is example 4.
Fig. 2 SEM pictures of samples with different alumina contents, wherein (2 a) is example 1, (2 b) is example 2, (2 c) is example 3, and (2 d) is example 4.
FIG. 3 corrosion rates for samples of different silicon carbide contents.
FIG. 4 corrosion rates for samples of different alumina contents.
FIG. 5 mechanical properties of samples with different silicon carbide contents.
FIG. 6 mechanical properties of samples of different alumina contents.
Detailed Description
The invention will be further described with reference to the drawings and examples.
1. 3DP preparation technology for improving strength and corrosion resistance of magnesium alloy
1) Mixing magnesium alloy powder, ceramic powder and carbide powder in certain proportion.
2) And (3) introducing the shape of the product to be printed into a computer control system, and printing the mixed powder and glue obtained in the step (1) in a 3D printer in an alternate spray forming mode to obtain a blank with the required shape. In the step 2), the mixed powder obtained in the step 1) is filled into a metal material cylinder in a 3D printer, the glue is filled into a glue material cylinder in the 3D printer, and the alternate spraying comprises the following steps: firstly, uniformly spreading a layer of alloy powder on a powder bed, spraying a layer of glue on the layer of alloy powder, spraying a layer of alloy powder on the glue layer, spraying a layer of glue, and alternately spraying the alloy powder and the glue to obtain the blank. The glue is water-based low-molecular alcohol glue.
3) Drying the blank obtained in the step 2), and degreasing and sintering at 300-450 ℃ in a protective atmosphere or in vacuum. In the step 3), the blank is dried in air at 60-120 ℃ for 2-6 hours. In the step 3), degreasing and sintering the dried blank for 1-6 hours at 300-450 ℃ in protective atmosphere or vacuum.
4) Sintering the blank obtained in the step 3) at a high temperature of 580-660 ℃ in a protective atmosphere or in vacuum, and cooling to room temperature. In the step 4), sintering the blank for 5-70 hours at 580-660 ℃ in protective atmosphere or vacuum. The shielding gas is inert gas.
2. High-strength corrosion-resistant magnesium alloy material
The high-strength corrosion-resistant magnesium alloy material is prepared by adopting the 3DP preparation process for improving the strength and corrosion resistance of the magnesium alloy, and comprises the following components in percentage by mass: ceramic powder or carbide powder 0.1-20wt% and the balance being magnesium alloy powder. Wherein the ceramic powder is alumina ceramic. The carbide powder is silicon carbide. The content of alumina in the alumina ceramic is more than 75wt%. The magnesium alloy is AZ91D type magnesium alloy.
Examples 1-5 were prepared according to the raw material ratios described in table 1 using the method of the present invention.
TABLE 1
| Examples | SiC content | Al 2 O 3 Content of | AZ91D content |
| Example 1 | 1 wt% | -- | Allowance of |
| Example 2 | 3 wt% | -- | Allowance of |
| Example 3 | 5 wt% | -- | Allowance of |
| Example 4 | 10 wt% | -- | Allowance of |
| Example 5 | -- | 1 wt% | Allowance of |
| Example 6 | -- | 3 wt% | Allowance of |
| Example 7 | -- | 5 wt% | Allowance of |
| Example 8 | -- | 10 wt% | Allowance of |
TABLE 2
| Examples | Compressive strength MPa | The corrosion rate is mm/year 25 DEG C |
| Example 1 | 363 | 85 |
| Example 2 | 389 | 51 |
| Example 3 | 420 | 92 |
| Example 4 | 332 | 224 |
| Example 5 | 359 | 82 |
| Example 6 | 380 | 56 |
| Example 7 | 288 | 158 |
| Example 8 | 190 | 366 |
As can be seen from fig. 1-2 and tables 1 and 2, as the amount of the ceramic powder or the carbide powder increases, the number of pores in the sample is obviously increased, and the corrosion rate of the sample is reduced and then increased, because the number of pores in the sample is smaller when the amount of the ceramic powder or the carbide powder is smaller, the second phase can effectively block the contact between the corrosion medium and the magnesium matrix, so that the corrosion rate is reduced; as the amount of ceramic or carbide powder increases, the number of voids in the sample increases and the corrosive medium and magnesium matrix again come into contact, causing the sample to erode at a progressively increasing rate. The compression strength is changed in a parabolic manner along with the increase of the consumption of the ceramic powder or the carbide powder, when the addition amount is small, the number of pores in the sample is small, the sample is more compact, and the added second phase can prevent the expansion of cracks, so that the compression strength of the sample is effectively improved; when the amount of addition is excessive, holes in the sample are increased, and cracks preferentially propagate through the holes, resulting in gradual decrease in mechanical strength of the sample. Therefore, the additive manufacturing process of sintering after glue bonding, printing and forming can effectively solve the problems of difficult processing of complex shapes, keep the advantage of weight reduction, have the advantages of low manufacturing cost, high production efficiency, wide application range and the like, can realize the feasibility of manufacturing magnesium alloy workpieces with large size and complex shapes, can mix other second materials in the magnesium alloy powder in any proportion, does not have the casting problems of segregation and the like, and has uniform final product components. Meanwhile, the process can densify different materials together after mixing, so that the magnesium alloy product with a complex shape can still keep higher strength and better corrosion resistance.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the technical solution, and those skilled in the art should understand that modifications and equivalents may be made to the technical solution of the present invention without departing from the spirit and scope of the present invention, and all such modifications and equivalents are included in the scope of the claims.
Claims (4)
1. The 3DP preparation process for improving the strength and corrosion resistance of the magnesium alloy is characterized by comprising the following steps of:
1) Uniformly mixing magnesium alloy powder, silicon carbide or aluminum oxide according to a proportion;
2) Introducing the shape of a product to be printed into a computer control system, and printing the mixed powder and glue obtained in the step 1) in a 3D printer in an alternate spray forming mode to obtain a blank with the required shape;
3) Drying the blank obtained in the step 2) in air at 60-120 ℃ for 2-6 hours, and degreasing and sintering at 350-430 ℃ for 1-6 hours in a protective atmosphere or vacuum;
4) Sintering the blank obtained in the step 3) in protective atmosphere or vacuum for 5-70 hours at 590-650 ℃ and cooling to room temperature;
the high-strength corrosion-resistant magnesium alloy material comprises the following components in percentage by mass: 1-10wt% of silicon carbide or aluminum oxide, and the balance of magnesium alloy powder; the magnesium alloy is AZ91D type magnesium alloy.
2. The 3DP manufacturing process for improving the strength and corrosion resistance of magnesium alloy according to claim 1, wherein in the step 2), the mixed powder obtained in the step 1) is loaded into a metal cylinder in a 3D printer, the glue is loaded into a glue cylinder in the 3D printer, and the alternate spraying comprises the following steps: firstly, uniformly spreading a layer of alloy powder on a powder bed, spraying a layer of glue on the layer of alloy powder, spraying a layer of alloy powder on the glue layer, spraying a layer of glue, and alternately spraying the alloy powder and the glue to obtain the blank.
3. The 3DP manufacturing process for improving the strength and corrosion resistance of magnesium alloy according to claim 1, wherein the shielding gas is an inert gas.
4. The 3DP preparation process for improving the strength and corrosion resistance of magnesium alloy according to claim 1, wherein the glue is water-based low molecular alcohol glue.
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| CN114603156A (en) * | 2022-04-11 | 2022-06-10 | 合肥工业大学智能制造技术研究院 | Method for preparing high-corrosion-resistance magnesium alloy by utilizing ink-jet 3D printing technology |
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| JPWO2021157748A1 (en) * | 2020-02-07 | 2021-08-12 |
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| CN110976846A (en) * | 2019-12-06 | 2020-04-10 | 重庆工港致慧增材制造技术研究院有限公司 | Magnesium-based composite material for 3D printing, preparation method and 3D printing method thereof |
| JPWO2021157748A1 (en) * | 2020-02-07 | 2021-08-12 | ||
| CN112974837A (en) * | 2021-02-09 | 2021-06-18 | 重庆大学 | Two-step sintering process method for 3D printing of magnesium alloy material |
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